Textile material



Patented Feb. 14, 1939 UNITED STATES PATENT OFFICE TEXTILE-MATERIALHerbert Platt and Arthur Lyem, Cumberland, Md., assignors to CelaneseCorporation of America, a corporation of Delaware No Drawing.Application January 21, 1937 Serial No. 121,596

9 Claims.

This invention relates to a new and improved process for the weightingof textile materials of whatsoever composition and more particularly tothe weighting of textile materials containing organic derivatives ofcellulose.

An object of the invention is to provide an The textile materialsweighted according to this invention present considerable advantagesover unweighted. materials. Thus, for example, there is a reduction inthe tendency of woven fabrics to slip, and circular knitted fabrics toladder and warp knitted fabrics to split, and an increase in thefullness or volume of the yarns, threads or fabrics resulting inimproved handle or feel. Moreover, by the process of the presentinvention there is efiected an economy in the material used to produce agood result. Forfexample, in a woven fabric less ends and picks per inchwill be needed to produce a good result than with unloaded materials.Furthermore, by-treating the fabrics in accordance with the instantinvention, their resistance to various agents such as heat in ironing orfinishing or aqueous treatments at high temperatures is increased, andtheir affinity for certain dyes is changed, especially in the case wheresynthetic fibres and filaments are employed.

Many methods have been devised, both here and abroad, for weightingfabrics made of or containing an organic derivative of cellulose. Mostof the methods, however, have been commercially unsatisfactory. Thedifliculty with most of the processes has been that the application ofthe weighting metal solution to the fabric has been accompanied byswelling or gelling of the fabric. The main difiiculty on a commercialscale has, therefore, .been to handle the fabric in the gelled orswollen condition. Only a very slightvariation intension on the fabricin the gelled or swollen condition is required to produce creases,wrinkles or streakiness in the dyed fabric. Various types of machinesand devices have been constructed to handle the fabric, but none hasbeen entirely successful from a commercial standpoint. By employing thisinvention, fabrics con- 55 taining an organic derivative of celluloseare weighted to as high as or moreof weight increase without materially.swelling or gelling the organic derivative of cellulose. This inventionpermits of .the handling of said fabrics in the manner necessary forcommercial production without producing defects such as creases,wrinkles, uneven stretching, etc. I

In accordance with this invention, we weight textile materials of anycomposition by treating them with a solution of a tin compound at anelevated temperature for a short period, treating them a second time ina similar bath at reduced temperature, then hydrolyzing, phosphating, I

silicating and/or otherwise converting the soluble compound of tin to aninsoluble compound of tin. Also, in accordance with our imvention, weweight fabrics containing an organic derivative of cellulose with anysuitable metallic weighting compound such as those containing tin,titanium,

zinc, antimony, etc. by treating the fabrics containing an organicderivative of cellulose for a short period in a heated bath containing asoluble compound of the weighting metal, then-treating said fabric in asecond bath of said weighting metal at a reduced temperature, thenhydrolyzing, phosphating, silicating or otherwise converting the solublemetal weighting compound to an insoluble compound of the metal.

The yarns, filaments, fibres or fabrics may be, made from pr contain anysuitable organic derivative of cellulose, such as the organic esters ofcellulose and cellulose ethers. Examples of the organic esters ofcellulose are cellulose acetate, celulose formate, cellulose propionateand cellulose butyrate, while examples of cellulose ethers are ethylcellulose, methyl cellulose and benzyl cellulose. Fibres, filaments oryarns made from yarns containing an organic derivative of cellulose maybe employed with fibres, filaments or yarns of other textile materialsto produce a fabricwhich may also be successfully treated in other typesof mixtures of fibres, filaments or yarns may be employed.

This invention is also applicable to the weighting of yarns, filaments,fibres or fabrics made from or containing an organic derivative ofcellulose ing of yarns, fibres, filaments r fabrics of other textilematerials, for instance, cotton, regenerated or reconstituted cellulosemade by the cuprammonium or viscose method, silk, wool and othervegetable or animal fibres.

In tin weighting of any textile material or the weighting of textilematerials containing an organic derivative of cellulose by any weightingmetal,the textile material is subjected to the treatment of a heatedsolution of the soluble weighting compound for, ashort period. Thetemperature of this solution is preferably between 30 and 70 C. fortextile materials containing an organic derivative of cellulose andbetween 30 and 100C. for some of the other types of textile materials.Prior to hydrolyzing, phosphating or silicating the thus treated textilematerial, it is preferable to pretreat said textile material in a bathof a composition similar to the first bath and maintained at or belowroom temperature to reduce the temperature of the textile material priorto exposure of same to the air or other reacting agents. It is alsopreferable to so carry out the process that the textile material isexposed to as little air as possible between the heated bath and thecool or cold bath. The cool or cold bath may be of any suitabletemperature belowv 25 C.

The textile materials are preferably treated in ahot bath and cool orcold bath containing the soluble weighting compound at a concentrationbetween 20 and 38 B. The duration of the treatment in a hot bath ispreferably from 0.5 to 4 minutes, while the treatment in the cool orcold bath is of a duration sufiicient to reduce I minutes. The textilematerials may be given,

1, 2 or any number of passages through the hot and cold baths of thesoluble weighting compound with or without converting the weightingchloride of 30 to 35. B. maintained at about 22 0. there is imparted tothe fabric from 18 to 22% of weight increase. Where, however, the

fabric is of regenerated cellulose and the conoentrations of the hot andcold baths are between 30 and 35 B., the weight increaseis from 20 to30%. In the case ofa silk fabric there'is imparted between 20 and 25%weight increase ,when the concentrations of the baths are betw en 20 and30 B., and in the case of a cotton f bric a to weight increase iseffected when the concentrations of the baths are between and 35 B. Fromthesepercentages the weight increase of fabrics formed from mixedtextile materials may readily be calculated. One passage of a celluloseacetatefabric through the heated and cooled baths of the solubleweighting metal compound, hydrolyzing, phosphating, and

silicating produces about weight increase, while a second passage raisesthe weight increase The hydrolyzing of the soluble weighting compoundmay be accomplishedby flushing the textile material with cold or warmwater. It is preferable in the case of tin weighting to flush thetextile material, for example, by means of sprays, with a hard watermaintained at about or below 20 C. The phosphating operation may beaccomplished byimmersion of the textile material for from 15 to 45minutes in a bath of sodium or other alkaline dior tri-phosphate. Theconcentration of the phosphating solution is preferably from 5.to 7 B.After the phosphating operation, it is preferable to wash the textile'material prior to a second passage" through the soluble ,veightingmetal compound or prior to silicating. The silicating treatmentpreferably consists in immersing the textile material for from 15 to 45minutes in 'a solution ofsodium or potassium silicate maintained at 55C.'and having a concentration of from 1.5 to 3.5 B. The textile materialafter being treated in the bath containing a soluble weighting metalcompound may be either phosphated or silicated or both. The textilematerial may be.,phosphated and then silicated or' silicated only.

Yarns, fibres, filaments or fabrics may be treated with the soluble'weighting metal compound by placing the textile material in bags orbaskets and dipping the same in a bath of the soluble weightingcompound. Yarns or threads may be treated in the weighting'baths byhank-dipping methods, or as yarns or threads continuously travellingthrough the baths, either as a single yarn or thread or as bundles,bands or ribbons of the yarns or threads. Fabrics are preferably treatedby a continuous process wherein the fabric in open width is drawnthrough the baths of the soluble weighting metal solution for a shortperiod at elevated temperature and then through a bath or baths toconvert the soluble weighting metal compound to the insoluble orrelatively insoluble state. The weighting baths are preferably soarranged that between the heated weighting bath and the cool or coldweighting bath the fabric is exposed to as little .air as possible.Furthermore, when employing the hydrolyzing step, the fabricshould' beflushed with water as soon as possible after leaving the cool or coldweighting. bath.

As one method of carrying out the invention, fabric in roll form may besupported'at one end of a series of tanks. The first tank may, forinstance, be 10 feet long, 4 to 8 inches deep and rubber lined; Thistank is provided with means to maintain the fabric submerged in thesame, and with means to maintain the desired temperature andconcentration of the solution therein. The fabric is drawn through andover the edge of the tank into a second'tank. The second tank may be,for instance, 2' feet long, rubber lined and'provided with means formaintaining the temperature and, concentration of the solution. From thesecond tank the fabric may pass over a roller and between a pair of niprollers into a water spray. From the water spray and further wash thefabric may be drawn through tanks in a circuitous manner equipped in asecond tank (which is the cold weighting tank) for 0.5 minute, under thewater spray for two minutes, in the third tank (which is the phosphatingor silicatlng bath) for 30 minutes and in the fourth tank, if desired,for asimilar period of time. After being removed from the last tank thefabric may be centrifuged, tenter' dried, ironed or otherwise dried andthen rerolled. Obviously, tanks of any length or construction may beemployed depending upon the speed of the fabrics being drawn through thesame.

As an illustration of the invention but without being limited thereto,the following example is given:

Example A fabric consisting of cellulose acetate is treated for 1 minuteat a speed of 3 to 5 yards per minute ina bath 30 times its weight ofstannic chloride having a concentration of 33 B., and at a temperatureof from 45 to 55 C. fabric is then treated with a cold bath maintainedat about to 20 C. of the same compound and' concentration for 0.33minute. It is found that this treatment in a cold bath prevents loss inhydrolyzing and in effect adds 3 to 20% more weighting to the fabric andgreatly increases the evenness with which the weighting compound isplaced in or on the fabric. The fabric is then passed through niprollers, sprayed with cold hard water to hydrolyze the tin. Thefabric'after further Washing is then immersed in a phosphating bathcontaining di-sodium phosphate of 6.5 B. for 20 minutes at 50 C. andthen washed. The fabric after phosphating is immersed for 30 minutes at55 C. in a 25 B. solution of sodium silicate and washed. The fabric isthen tenter dried. The fabric is found to be evenly weighted 'to aweight increase of about 25%. The strength of the fabric is equal tothat of the fabric before treatment and there are present no wrinklesdue to stretching, or unevenness of dye aflinity due to the unevenstretching in handling of gelled or swollen yards.

The term weighting is used in the appended claims in the ordinarytechnical signification in which it is employed in connection withnatural silk. That is to say, to denote the operation of increasing theweight and volume of the material under treatment; it does not includethe production of such relatively small increases in weight as may beassociated with processes of dyeing, such as, for example, thoseeffected with the aid of mordants.

It is to be understood that the foregoing detailed description is givenmerely by way of illustration and that many variations may be madetherein without departing from the spirit of our invention.

Having described our invention, what we desire to secure by LettersPatent is:

1. In a process for weighting textile material without substantiallyswelling or gelling the material, the steps of impregnating the materialwith a solution of a soluble weighting metal compound at a temperatureabove 45 C. and cooling the impregnated material in a solution of thesame weighting metal compound maintained at a temperature below 25 0.,and subsequently fixing the metal in said textile material as aninsoluble compound.

2. Process forweighting textile material con- The Y taining organicderivatives of cellulose Without substantially swelling or gelling thematerial, which comprises impregnating the material with a solution of asoluble weighting metal'compound at a temperature above 45v C., coolingthe impregnated material in a solution of the same weighting metalcompound maintained at a temperature below 25 C., and subsequentlyfixing the metal in said textile-material as an insoluble compound.

3. Process for weighting textile material containing cellulose acetatewithout substantially swelling or gelling the. material, which comprisesimpregnating the material with a solution of a soluble weighting metalcompound at a temperature above 45 0., cooling the impregnated materialin a solution of the same weighting metal compound maintained at atemperature below 25 C. and subsequently fixing the metal in saidtextile material as an insoluble compound. g

4. Process for weighting'textile material containing organic derivativesof cellulose without substantially swelling or gelling the material,which comprises impregnating the material with a solution of a solubleweighting metal compound at a temperature above 45 0., cooling theimpregnated material in a solution of the same weighting metal compoundmaintained at a temperature below 25 C., and subsequently fixing themetal in said textile material as an insoluble compound by treatmentwith cold water and a solution of a compound selected from the groupconsisting of alkaline phosphates and alkaline silicates.

5. Process for weighting textile material containing cellulose acetatewithout substantially swelling or gelling the material, which comprisesimpregnating the material with a solution of a soluble weighting metalcompound at a temperature above 45 C., cooling the impregnated materialin a solution of the same weighting metal compound maintained .at atemperature below 25 C., and subsequently fixing the metal in saidtextile material as an insoluble compound by treatment with cold waterand a solution of a compound selected from the group consisting ofalkaline phosphates and alkaline silicates.

6. Process for weighting textile materials containing organicderivatives of cellulose without substantially swelling or gelling thematerial, which comprises impregnating the material with a solutionoftin chloride by treating the material with a solution of tin chlorideof 20 to 28 Baum at a temperature above 45 C. for from swelling orgelling the material, which comprises impregnating the material with asolution of tin chloride by treating the material with a solution of tinchloride of 20 to 38 Baum at a temperature above 45 C. for from /2 to 4-minutes, cooling the impregnated material by treating the same from A to1 /2 minutes with a solution of tin chloride maintained at a temperaturebelow 25 C and subsequently fixing the metal in said material as aninsoluble compound.

8. Process for weighting textile materials containing organicderivatives of cellulose without to 4 minutes, cooling the impregnatedmaterial by treating the same from A; to 1 /2 minutes with a solution oftin chloride maintained at a temperature below 25 0., and subsequentlyfixing the metal in said material as an insoluble compound by treatmentwith cold water and a solution of a compound selected from the groupconsisting of alkaline phosphates and alkaline silicates.

9. Process for weighting textile materials containing cellulose acetatewithout substantially Patent No. 2,1i .7,056.

CERTIFICATE OF CORRECTION.

HERBERT PLAT'I', ET AL,

swelling or gelling the material, which comprises impregnating thematerial with a solution of tin chloride by treating the material with asolution of tin chloride of to 38 Baum at a temperature above C. forfrom /2 to 4 minutes, cooling the impregnated material by treating thesame from $4; to 1 /2 minutes with a solution of tin chloride maintainedat a temperature be- .low 25 C. and subsequently fixing the metal insaid material as an insoluble compound by treatment with cold water anda solution of a compound selected from the group consisting of alkalinephosphates and alkaline silicates.

HERBERT PhA'I'r. ARTHUR LYEM.

February 1h, 1959s It is hereby certified that error appears intheprinted specification of the above numbered patent requiring correctionas follows: Pagerl, second colunln, line 8, for the word 'or read of;page 2, first co1mnn,- line 59, for "chloride of to B." read compositionand strength; page 3, second column, line 51 claini 6, for "28" read 38;and that the said Letters Patent should be read with this correctiontherein that the same may conform to the record of the case in thePatent Office Signed and sealed this 1 th day r April, A D. 19590 (Seal)Henry Van Arsdale Acting Commissioner of Patentso

